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Diffraction techniques
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Series: ASM Handbook
Volume: 11B
Publisher: ASM International
Published: 15 May 2022
DOI: 10.31399/asm.hb.v11B.a0006931
EISBN: 978-1-62708-395-9
Abstract
This article presents tools, techniques, and procedures that engineers and material scientists can use to investigate plastic part failures. It also provides a brief survey of polymer systems and the key properties that need to be measured during failure analysis. It describes the characterization of plastics by infrared and nuclear magnetic resonance spectroscopy, differential scanning calorimetry, differential thermal analysis, thermogravimetric analysis, thermomechanical analysis, and dynamic mechanical analysis. The article also discusses the use of X-ray diffraction for analyzing crystal phases and structures in solid materials.
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.9781627082952
EISBN: 978-1-62708-295-2
Series: ASM Handbook
Volume: 11
Publisher: ASM International
Published: 15 January 2021
DOI: 10.31399/asm.hb.v11.a0006768
EISBN: 978-1-62708-295-2
Abstract
X-ray diffraction (XRD) residual-stress analysis is an essential tool for failure analysis. This article focuses primarily on what the analyst should know about applying XRD residual-stress measurement techniques to failure analysis. Discussions are extended to the description of ways in which XRD can be applied to the characterization of residual stresses in a component or assembly and to the subsequent evaluation of corrective actions that alter the residual-stress state of a component for the purposes of preventing, minimizing, or eradicating the contribution of residual stress to premature failures. The article presents a practical approach to sample selection and specimen preparation, measurement location selection, and measurement depth selection; measurement validation is outlined as well. A number of case studies and examples are cited. The article also briefly summarizes the theory of XRD analysis and describes advances in equipment capability.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006643
EISBN: 978-1-62708-213-6
Abstract
This article describes the methods of X-ray diffraction analysis, the types of information that can be obtained, and its interpretation. The discussion covers the basic theories of X-rays and various types of diffraction experiments, namely single-crystal methods for polychromatic and monochromatic beams, powder diffraction methods, and the Rietveld method.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006680
EISBN: 978-1-62708-213-6
Abstract
X-ray powder diffraction (XRPD) techniques are used to characterize samples in the form of loose powders, aggregates of finely divided material or polycrystalline specimens. This article provides a detailed account of XRPD. It begins with a discussion on XRPD instrumentation and the techniques used to characterize samples. The article then describes the principles, advantages, and disadvantages of various types of powder diffractometers. A section on the Rietveld method of diffraction analysis is then presented. The article discusses various methods and procedures for qualifying and quantifying phase mixtures in powder samples. It provides information on typical sensitivity and experimental limits on precision of XRPD analysis and other systematic sources of errors that affect accuracy. Some of the factors pertinent to the estimation of crystallite size and defects are also presented. The article ends with a few application examples of XRPD.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006631
EISBN: 978-1-62708-213-6
Abstract
This article provides a detailed account of the concepts of single-crystal x-ray diffraction (XRD). It begins with a historical review of XRD methods, followed by a description of the various factors involved in crystal symmetry. The article then focuses on the phase problem in x-ray structural analysis and validation of the structural model. Some of the factors to be considered for performing experimental procedure are provided. The article presents several examples of applications of single-crystal XRD. The following sections cover the crystallographic problem in terms of structural analysis, software programs for crystal structure solution and refinement, and visualization of crystal structures. The article ends with a discussion on various databases available for single-crystal XRD analysis.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006656
EISBN: 978-1-62708-213-6
Abstract
This article discusses various concepts of micro x-ray diffraction (XRD) used for the examination of materials in situ. The discussion covers the principles, equipment used, sample preparation procedure, considerations for calibrating a detector, steps for performing data analysis, and applications and interpretation of micro-XRD.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006632
EISBN: 978-1-62708-213-6
Abstract
This article provides a detailed account of x-ray diffraction (XRD) residual-stress techniques. It begins by describing the principles of XRD stress measurement, followed by a discussion on the most common methods of XRD residual-stress measurement. Some of the procedures required for XRD residual-stress measurement are then presented. The article provides information on measurement of subsurface stress gradients and stress relaxation caused by layer removal. The article concludes with a section on examples of applications of XRD residual-stress measurement that are typical of industrial metallurgical, process development, and failure analysis investigations undertaken at Lambda Research.
Book Chapter
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006654
EISBN: 978-1-62708-213-6
Abstract
This article discusses the techniques and applications of synchrotron x-ray diffraction, providing information on x-ray generation, monochromation, and crystallography. X-ray diffraction techniques covered include single-crystal and powder diffraction. Some of the factors involved in the construction and development of macromolecular x-ray crystallography are also described.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006660
EISBN: 978-1-62708-213-6
Abstract
The electron backscatter diffraction (EBSD) technique has proven to be very useful in the measurement of crystallographic textures, orientation relationships between phases, and both plastic and elastic strains. This article focuses on backscatter diffraction in a scanning electron microscope and describes transmission Kikuchi diffraction. It begins with a discussion on the origins of EBSD and the collection of EBSD patterns. This is followed by sections providing information on EBSD spatial resolution and system operation of EBSD. Various factors pertinent to perform an EBSD experiment are then covered. The article further describes the processes involved in sample preparation that are critical to the success or usefulness of an EBSD experiment. It also discusses the applications of EBSD to bulk samples and the development of EBSD indexing methods.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006681
EISBN: 978-1-62708-213-6
Abstract
Transmission electron microscopy (TEM) approach enables essentially simultaneous examination of microstructural features through imaging from lower magnifications to atomic resolution and the acquisition of chemical and crystallographic information from small regions of the thin specimen. This article discusses fundamentals of the technique, especially for solving materials problems. Background information is provided to help understand basic operations and principles, including instrumentation, the physics of signal generation and detection, image formation, electron diffraction, and spectrometry techniques with data analysis.
Series: ASM Handbook
Volume: 10
Publisher: ASM International
Published: 15 December 2019
DOI: 10.31399/asm.hb.v10.a0006655
EISBN: 978-1-62708-213-6
Abstract
Low-energy electron diffraction (LEED) is a technique for investigating the crystallography of surfaces and overlayers adsorbed on surfaces. This article provides a brief account of LEED, covering the principles and measurements of diffraction from surfaces. Some of the processes involved in sample preparation are described. In addition, the article discusses the limitations of surface-sensitive electron diffraction and the applications of LEED with examples.
Series: ASM Handbook
Volume: 17
Publisher: ASM International
Published: 01 August 2018
DOI: 10.31399/asm.hb.v17.a0006472
EISBN: 978-1-62708-190-0
Abstract
Time-of-flight diffraction (TOFD) is an ultrasonic technique used to detect diffracted waves from crack tips and to size the cracks from the arrival times of those waves. This article discusses the basic considerations and provides information on probe selection, gain setting, and instrumentation of TOFD. It describes the numerous effects that result from modifying the probe characteristics. The article provides the American Society of Mechanical Engineers (ASME), the European Committee for Standardization (CEN), and the International Standardization Organization (ISO) recommendations for the reference blocks according to applicable codes and standards. It also provides the ASME, CEN, and ISO recommendations for examination of welds. The article concludes with information on the interpretation and analysis of TOFD images with an aid of sizing algorithms.
Book: Powder Metallurgy
Series: ASM Handbook
Volume: 7
Publisher: ASM International
Published: 30 September 2015
DOI: 10.31399/asm.hb.v07.a0006126
EISBN: 978-1-62708-175-7
Abstract
This article discusses the capabilities and limitations of various material characterization methods that assist in the selection of a proper analytical tool for analyzing particulate materials. Commonly used methods are microanalysis, surface analysis, and bulk analysis. The techniques used for performing microanalysis include scanning electron microscopy and electron probe X-ray microanalysis. The article describes surface analysis techniques, including Auger electron spectroscopy, X-ray photoelectron spectroscopy, and ion-scattering spectroscopy. Bulk analysis techniques, such as X-ray powder diffraction, inductively coupled plasma atomic emission spectroscopy, atomic absorption spectroscopy, and atomic fluorescence spectrometry, are also discussed.
Book: Powder Metallurgy
Series: ASM Handbook
Volume: 7
Publisher: ASM International
Published: 30 September 2015
DOI: 10.31399/asm.hb.v07.a0006096
EISBN: 978-1-62708-175-7
Abstract
Particle size and size distribution have a significant effect on the behavior of metal powders during their processing. This article provides an overview of the sample preparation process for particle size measurement, which is a key step in the measurement of particle size distributions. Common particle size measuring techniques discussed in this article include sieve analysis, quantitative image analysis, laser diffraction, sedimentation methods, aerodynamic time-of-flight method, electrical zone sensing, and photon correlation spectroscopy. The advantages and disadvantages of these methods are reviewed.
Book: Thermal Spray Technology
Series: ASM Handbook
Volume: 5A
Publisher: ASM International
Published: 01 August 2013
DOI: 10.31399/asm.hb.v05a.a0005731
EISBN: 978-1-62708-171-9
Abstract
The raw materials used in thermal spray processes are a critical parameter in the finished coating because the variations in their size, morphology, chemistry, and phase composition can significantly impact coating properties. Therefore, it is important to test and characterize the raw materials. This article discusses various characterization methods for powders. Topics discussed include: methods for determining particle size and/or size distribution; powder and coating stoichiometry; particle chemistry; and phase analysis by x-ray diffraction. This article discusses the characterization of thermal spray powders which involves the determination of particle size and/or size distribution and phase analysis by x-ray diffraction. It provides information on preferential volatilization and rapid solidification that influence compositional differences. Wet chemical methods, spectographic analysis, and atomic absorption spectrometry are also discussed.
Series: ASM Handbook
Volume: 22B
Publisher: ASM International
Published: 01 November 2010
DOI: 10.31399/asm.hb.v22b.a0005532
EISBN: 978-1-62708-197-9
Abstract
This article discusses the central aspect of anisotropy modeling, namely, texture measurement and analysis. It provides an overview of the methods available for characterizing crystallographic preferred orientation, or texture, in polycrystalline materials. These methods include pole figure measurement and electron backscatter diffraction (EBSD). The article describes the process considerations for pole figure measurement, including X-ray diffraction, neutron diffraction, stereographic projection, equal area projection, graphing pole figures, typical textures, and orientation distribution. It also deals with the limitations and challenges associated with the EBSD, and applications of the diffraction.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003528
EISBN: 978-1-62708-180-1
Abstract
This article focuses primarily on what an analyst should know about applying X-ray diffraction (XRD) residual stress measurement techniques to failure analysis. Discussions are extended to the description of ways in which XRD can be applied to the characterization of residual stresses in a component or assembly. The article describes the steps required to calibrate instrumentation and to validate stress measurement results. It presents a practical approach to sample selection and specimen preparation, measurement location selection, and measurement depth selection, as well as an outline on measurement validation. The article also provides information on stress-corrosion cracking and corrosion fatigue. The importance of residual stress in fatigue is described with examples. The article explains the effects of heat treatment and manufacturing processes on residual stress. It concludes with a section on the XRD stress measurements in multiphase materials and composites and in locations of stress concentration.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003520
EISBN: 978-1-62708-180-1
Abstract
This article outlines the basic steps to be followed and the range of techniques available for failure analysis, namely, background data assembling, visual examination, microfractography, chemical analysis, metallographic examination, electron microscopy, electron microprobe analysis, X-ray techniques, and simulations. It also describes the steps for analyzing the data, preparing the report, preservation of evidence, and follow-up on recommendations.
Series: ASM Handbook Archive
Volume: 11
Publisher: ASM International
Published: 01 January 2002
DOI: 10.31399/asm.hb.v11.a0003529
EISBN: 978-1-62708-180-1
Abstract
This article describes some of the common elemental composition analysis methods and explains the concept of referee and economy test methods in failure analysis. It discusses different types of microchemical analyses, including backscattered electron imaging, energy-dispersive spectrometry, and wavelength-dispersive spectrometry. The article concludes with information on specimen handling.
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